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HRID 20840作成日:2026年10月24日

1,2-Dichloroethane → HCID 59347881、化合物

https://huagongshe.com/ja/reaction/20840

反応式

関与物質

役割名称HCID仕込み量
反応物1,2-DichloroethaneHCID 11—
反応物1-HydroxybenzotriazoleHCID 75771—
反応物Sodium BicarbonateHCID 516892—
反応物2-Chloro-3-(trifluoromethyl)benzoic acidHCID 2736677—
反応物[2-Methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amineHCID 59347786—
溶媒DichloromethaneHCID 6344—
生成物HCID 59347881HCID 59347881—

反応手順

A mixture of [2-methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amine D26 (0.150 g; 0.647 mmol), 2-chloro-3-(trifluoromethyl)benzoic acid (0.174 g; 0.775 mmol), EDC (0.149 g; 0.777 mmol) and HOBt (0.020 g; 0.148 mmol) in DCM (4 ml) was shaken at room temperature for 66 hours. Saturated sodium hydrogen carbonate (8 ml) was added and shaking continued for 0.5 hours. The organic layer was passed through a phase separation cartridge and applied to a 2 g SCX column. The column was washed with DCM and methanol and the product eluted with 1M ammonia in methanol. The crude product was purified by chromatography on silica gel (20 g) eluting with 0-100% ethyl acetate in pentane gradient to afford the title compound as two pairs of enantiomers.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07745642B2
出典データセットuspto-grants-2010_06
ORD IDord-d442d140b910474784016bfda8a268a9
出典メモuspto-grants-2010_06